反应详情

To a stirred solution of methyl 4-[1-(tert-butoxycarbonyl)-4-(2,4-difluorophenoxy)-2-pyrrolidinylmethoxy]benzoate (529 mg, 1.15 mmol) in CH2Cl2 (5 ml) was added TFA (5 ml). The mixture was stirred overnight. The mixture was concentrated in vacuo and the residue was made basic by the addition of sat. NaHCO3. The mixture was extracted with CHCl3 (2×100 ml). The extracts were dried over K2CO3 and evaporated to give methyl 4-[4-(2,4-difluorophenoxy)-2-pyrrolidinylmethoxy]benzoate (385 mg, 92%) as a yellow oil. 1H-NMR (CDCl3) δ1.89-1.95 (m, 1 H), 2.28-2.35 (m, 1 H), 3.09 (dd, J=12.5, 4.9 Hz, 1 H), 3.33 (d, J=12.5 Hz, 1 H), 3.60 (m, 1 H), 3.86 (s, 3 H), 4.10 (d, J=5.6 Hz, 2 H), 4.84 (m, 1 H), 6.73-6.89 (m, 3 H), 6.91 (d, J=8.5 Hz, 2 H), 7.96 (d, J=8.5 Hz, 2 H).

1. concentrationThe mixture was concentrated in vacuo
2. additionthe residue was made basic by the addition of sat. NaHCO3
3. extractionThe mixture was extracted with CHCl3 (2×100 ml)
4. dry with materialThe extracts were dried over K2CO3
5. customevaporated